KR20210003755A - Polishing agent for synthetic quartz glass substrates, manufacturing method thereof, and polishing method for synthetic quartz glass substrates - Google Patents
Polishing agent for synthetic quartz glass substrates, manufacturing method thereof, and polishing method for synthetic quartz glass substrates Download PDFInfo
- Publication number
- KR20210003755A KR20210003755A KR1020207030435A KR20207030435A KR20210003755A KR 20210003755 A KR20210003755 A KR 20210003755A KR 1020207030435 A KR1020207030435 A KR 1020207030435A KR 20207030435 A KR20207030435 A KR 20207030435A KR 20210003755 A KR20210003755 A KR 20210003755A
- Authority
- KR
- South Korea
- Prior art keywords
- polishing
- quartz glass
- synthetic quartz
- abrasive
- glass substrate
- Prior art date
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 150
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000000758 substrate Substances 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims description 30
- 239000003795 chemical substances by application Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000002245 particle Substances 0.000 claims abstract description 101
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 48
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 29
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 9
- -1 rare earth salt Chemical class 0.000 claims description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 11
- 239000004202 carbamide Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000007517 polishing process Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- 238000007788 roughening Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 43
- 239000000243 solution Substances 0.000 description 37
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 20
- 150000002500 ions Chemical class 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 239000011164 primary particle Substances 0.000 description 16
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 15
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 15
- LENJPRSQISBMDN-UHFFFAOYSA-N [Y].[Ce] Chemical compound [Y].[Ce] LENJPRSQISBMDN-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 10
- 239000008119 colloidal silica Substances 0.000 description 9
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 239000003637 basic solution Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 230000000996 additive effect Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 4
- 239000006061 abrasive grain Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000000703 Cerium Chemical class 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000001014 amino acid Nutrition 0.000 description 2
- 229940024606 amino acid Drugs 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 description 1
- UWHSPZZUAYSGTB-UHFFFAOYSA-N 1,1,3,3-tetraethylurea Chemical compound CCN(CC)C(=O)N(CC)CC UWHSPZZUAYSGTB-UHFFFAOYSA-N 0.000 description 1
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 description 1
- ZVWHURINXJWEER-UHFFFAOYSA-N 1,1,3,3-tetraphenylurea Chemical compound C=1C=CC=CC=1N(C=1C=CC=CC=1)C(=O)N(C=1C=CC=CC=1)C1=CC=CC=C1 ZVWHURINXJWEER-UHFFFAOYSA-N 0.000 description 1
- COSWCAGTKRUTQV-UHFFFAOYSA-N 1,1,3-trimethylurea Chemical compound CNC(=O)N(C)C COSWCAGTKRUTQV-UHFFFAOYSA-N 0.000 description 1
- HKQGDIKHDDGEOE-UHFFFAOYSA-N 1,1,3-triphenylurea Chemical compound C=1C=CC=CC=1N(C=1C=CC=CC=1)C(=O)NC1=CC=CC=C1 HKQGDIKHDDGEOE-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical group C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 239000004475 Arginine Substances 0.000 description 1
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 1
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 1
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 description 1
- DCXYFEDJOCDNAF-REOHCLBHSA-N L-asparagine Chemical compound OC(=O)[C@@H](N)CC(N)=O DCXYFEDJOCDNAF-REOHCLBHSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 description 1
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 description 1
- AGPKZVBTJJNPAG-WHFBIAKZSA-N L-isoleucine Chemical compound CC[C@H](C)[C@H](N)C(O)=O AGPKZVBTJJNPAG-WHFBIAKZSA-N 0.000 description 1
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 description 1
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 description 1
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- ROHFNLRQFUQHCH-UHFFFAOYSA-N Leucine Natural products CC(C)CC(N)C(O)=O ROHFNLRQFUQHCH-UHFFFAOYSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 description 1
- 239000004473 Threonine Substances 0.000 description 1
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 description 1
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 235000004279 alanine Nutrition 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 1
- 235000009582 asparagine Nutrition 0.000 description 1
- 229960001230 asparagine Drugs 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- GHDLZGOOOLEJKI-UHFFFAOYSA-N benzenesulfonylurea Chemical compound NC(=O)NS(=O)(=O)C1=CC=CC=C1 GHDLZGOOOLEJKI-UHFFFAOYSA-N 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 description 1
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- AGPKZVBTJJNPAG-UHFFFAOYSA-N isoleucine Natural products CCC(C)C(N)C(O)=O AGPKZVBTJJNPAG-UHFFFAOYSA-N 0.000 description 1
- 229960000310 isoleucine Drugs 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- BSJVXAGXBJYPJZ-UHFFFAOYSA-N n-carbamoyl-2-methylpropanamide Chemical compound CC(C)C(=O)NC(N)=O BSJVXAGXBJYPJZ-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
- B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
- B24B7/24—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding or polishing glass
- B24B7/241—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
본 발명은, 연마입자 및 물을 포함하는, 합성석영유리기판용의 연마제로서, 상기 연마입자가, 세륨과 이트륨의 복합산화물입자로서, 상기 연마입자 중에 함유되는 상기 세륨의 함유율이 71mol% 이상 79mol% 이하인 것을 특징으로 하는 합성석영유리기판용의 연마제이다. 이로 인해, 연마속도를 저하시키는 일 없이, 연마에 의한 합성석영유리기판 표면의 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판용의 연마제가 제공된다.The present invention is an abrasive for a synthetic quartz glass substrate comprising abrasive particles and water, wherein the abrasive particles are composite oxide particles of cerium and yttrium, and the content of the cerium contained in the abrasive particles is 71 mol% or more and 79 mol. It is an abrasive for synthetic quartz glass substrates, characterized in that it is not more than %. For this reason, there is provided an abrasive for a synthetic quartz glass substrate capable of sufficiently reducing the occurrence of defects on the surface of a synthetic quartz glass substrate due to polishing without lowering the polishing rate.
Description
본 발명은, 합성석영유리기판용의 연마제 및 그의 제조방법, 그리고 이 연마제를 사용한 합성석영유리기판의 연마방법에 관한 것이다.The present invention relates to an abrasive for a synthetic quartz glass substrate, a method for manufacturing the same, and a method for polishing a synthetic quartz glass substrate using the abrasive.
최근, 광리소그래피에 의한 패턴의 미세화에 의해, 합성석영유리기판의 결함밀도나 결함사이즈, 면거칠기, 평탄도 등의 품질에 관해, 한층 엄격한 것이 요구되고 있다. 그 중에서도 기판 상의 결함에 관해서는, 집적회로의 고정세화, 자기미디어의 고용량화에 수반하여, 추가적인 고품질화가 요구되고 있다.In recent years, with the miniaturization of patterns by photolithography, there is a demand for more stringent quality such as defect density, defect size, surface roughness, and flatness of a synthetic quartz glass substrate. Among them, with regard to defects on the substrate, high definition of integrated circuits and high capacity of magnetic media are required, and additional high quality is required.
이러한 관점에서, 합성석영유리기판용 연마제에 대해서는, 연마 후의 석영유리기판의 품질향상을 위해, 연마 후의 석영유리기판의 표면거칠기가 작은 것이나, 연마 후의 석영유리기판 표면에 스크래치 등의 표면결함이 적은 것이 강하게 요구되고 있다.From this point of view, with respect to the polishing agent for synthetic quartz glass substrate, the surface roughness of the quartz glass substrate after polishing is small in order to improve the quality of the quartz glass substrate after polishing, and the surface defects such as scratches on the surface of the quartz glass substrate after polishing are small. It is strongly demanded.
종래, 합성석영유리를 연마하기 위한 연마제로서, 실리카계의 연마제가 일반적으로 검토되고 있다. 실리카계의 슬러리는, 실리카입자를 사염화규소의 열분해에 의해 입성장시키고, 나트륨 등의 알칼리금속을 포함하지 않는 알칼리용액으로 pH조정을 행하여 제조하고 있다. 예를 들어, 특허문헌 1에서는, 고순도의 콜로이달실리카를 중성 부근에서 사용하여 결함을 저감할 수 있는 것이 기재되어 있다. 그러나, 콜로이달실리카의 등전점을 고려하면, 중성 부근에 있어서 콜로이달실리카는 불안정하여, 연마 중 콜로이달실리카지립의 입도분포가 변동되어 안정적으로 사용할 수 없게 되는 문제가 우려되고, 연마제를 순환 및 반복하여 사용하는 것이 곤란하여, 일회용으로 사용하기 때문에 경제적으로 바람직하지 않은 문제가 있다. 또한, 특허문헌 2에서는, 평균일차입자경이 60nm 이하인 콜로이달실리카와 산을 함유한 연마제를 사용함으로써, 결함을 저감할 수 있는 것이 기재되어 있다. 그러나, 이들 연마제는 현상의 요구를 만족시키기에는 불충분하여, 개량이 필요시된다.Conventionally, as an abrasive for polishing synthetic quartz glass, a silica-based abrasive has been generally studied. The silica-based slurry is prepared by granulating silica particles by thermal decomposition of silicon tetrachloride and adjusting the pH with an alkali solution containing no alkali metal such as sodium. For example, in
한편, 세리아(CeO2)입자는, 강산화제로서 알려져 있고, 화학적으로 활성인 성질을 갖고 있으므로 콜로이달실리카에 비해, 유리 등의 무기절연체의 연마속도향상에 유효하다(특허문헌 3, 4).On the other hand, ceria (CeO 2 ) particles are known as strong oxidizing agents and have chemically active properties, so they are effective in improving the polishing rate of inorganic insulators such as glass as compared to colloidal silica (Patent Documents 3 and 4).
그러나, 일반의 세리아계 연마제에서는, 건식 세리아입자가 사용되고, 건식 세리아입자는, 부정형인 결정형상을 갖고 있어, 연마제에 적용한 경우, 구형의 콜로이달실리카와 비교하여, 석영유리기판 표면에 스크래치 등의 결함이 발생하기 쉬운 문제가 있다. 또한, 세리아계 연마제는, 콜로이달실리카에 비해 분산안정성이 나쁘고, 입자가 침강하기 쉬운 문제도 있다.However, in general ceria-based abrasives, dry ceria particles are used, and dry ceria particles have an irregular crystal shape. When applied to an abrasive, compared to spherical colloidal silica, scratches on the surface of the quartz glass substrate There is a problem prone to defects. In addition, the ceria-based abrasive has poor dispersion stability compared to colloidal silica, and there is also a problem in that the particles are likely to settle.
합성석영유리기판의 세리아계 연마제로서, 건식 세리아입자를 대신하여 다면체결정형상인 습식 세리아입자를 사용한 경우, 스크래치 등의 결함은 건식 세리아입자에 비해 저감되었으나, 요구를 만족시킬 정도까지는 저감되지 않았다. 또한, 습식 세리아입자는 콜로이달실리카에 비해 경도가 딱딱한 점도 결함이 발생하기 쉬운 원인이다.In the case of using wet ceria particles having a polyhedral crystal shape instead of dry ceria particles as the ceria-based abrasive for the synthetic quartz glass substrate, defects such as scratches were reduced compared to the dry ceria particles, but not to the extent to satisfy the requirements. In addition, wet ceria particles have a harder viscosity than colloidal silica, which is the reason for the prone to occurrence of viscosity defects.
본 발명은 전술한 바와 같은 문제를 감안하여 이루어진 것으로, 연마속도를 저하시키는 일 없이, 연마에 의한 합성석영유리기판 표면의 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판용의 연마제 및 그의 제조방법을 제공하는 것을 목적으로 한다. 또한, 높은 연마속도를 갖고, 연마에 의한 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판의 연마방법을 제공하는 것도 목적으로 한다.The present invention has been made in view of the above-described problems, and is capable of sufficiently reducing the occurrence of defects on the surface of a synthetic quartz glass substrate due to polishing without lowering the polishing rate, and an abrasive for a synthetic quartz glass substrate and manufacture thereof It aims to provide a method. Another object of the present invention is to provide a method for polishing a synthetic quartz glass substrate having a high polishing rate and capable of sufficiently reducing the occurrence of defects due to polishing.
상기 목적을 달성하기 위해, 본 발명에서는, 연마입자 및 물을 포함하는, 합성석영유리기판용의 연마제로서, 상기 연마입자가, 세륨과 이트륨의 복합산화물입자로서, 상기 연마입자 중에 함유되는 상기 세륨의 함유율이 71mol% 이상 79mol% 이하인 것을 특징으로 하는 합성석영유리기판용의 연마제를 제공한다.In order to achieve the above object, in the present invention, as an abrasive for a synthetic quartz glass substrate comprising abrasive particles and water, the abrasive particles are composite oxide particles of cerium and yttrium, and the cerium contained in the abrasive particles. It provides an abrasive for a synthetic quartz glass substrate, characterized in that the content of 71 mol% or more and 79 mol% or less.
이러한 연마입자를 포함하는 연마제이면, 높은 연마속도를 가짐과 함께, 연마에 의한 합성석영유리기판 표면의 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판용의 연마제가 된다.An abrasive containing such abrasive particles is an abrasive for a synthetic quartz glass substrate capable of sufficiently reducing the occurrence of defects on the surface of a synthetic quartz glass substrate by polishing while having a high polishing rate.
또한, 상기 연마입자는 소성처리를 행하지 않은 입자인 것이 바람직하다.Further, it is preferable that the abrasive particles are particles that have not undergone firing treatment.
이와 같이 소성처리를 행하지 않은 연마입자는, 상술한 건식 세리아입자의 문제를 회피할 수 있다.The abrasive grains not subjected to the firing treatment as described above can avoid the above-described problem of dry ceria grains.
나아가, 상기 연마입자 중에 함유되는 상기 세륨의 함유량이 73mol% 이상 76mol% 이하인 것이 바람직하다.Further, it is preferable that the content of the cerium contained in the abrasive particles is 73 mol% or more and 76 mol% or less.
이러한 연마입자를 포함하는 연마제이면, 높은 연마속도를 가짐과 함께, 연마에 의한 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판용의 연마제로서 특히 호적하게 이용된다.An abrasive containing such abrasive particles is particularly suitably used as an abrasive for synthetic quartz glass substrates capable of sufficiently reducing the occurrence of defects due to polishing while having a high polishing rate.
또한, 본 발명은, 상기 합성석영유리기판용의 연마제의 제조방법으로서, 상기 연마입자를, 희토류염과, 과잉의 알칼리 화합물과의 습식 침전법에 의해 제조하는 것을 특징으로 하는 합성석영유리기판용의 연마제의 제조방법을 제공한다.In addition, the present invention is a method for producing the abrasive for a synthetic quartz glass substrate, characterized in that the abrasive particles are produced by a wet precipitation method of a rare earth salt and an excess alkali compound. It provides a method for producing an abrasive of.
이리하여, 입경이 균일한 입자를 제조할 수 있고, 이와 같이 하여 제조된 연마제를 이용함으로써, 연마에 의한 결함의 발생을 충분히 저감할 수 있다.In this way, particles having a uniform particle diameter can be produced, and the occurrence of defects due to polishing can be sufficiently reduced by using the thus produced abrasive.
이때, 상기 희토류염을 희토류의 질산염으로 하고, 상기 알칼리 화합물을 요소 또는 요소계의 화합물로 하는 것이 바람직하다.At this time, it is preferable to use the rare earth salt as a rare earth nitrate and the alkali compound as a urea or urea compound.
이리하여 효율 좋게 연마입자를 석출시킬 수 있다.In this way, abrasive particles can be efficiently deposited.
나아가, 본 발명은, 조연마(粗硏磨)공정과 이 조연마공정 후의 최종연마공정을 갖는 합성석영유리기판의 연마방법으로서, 상기 최종연마공정에 있어서, 상기 본 발명의 합성석영유리기판용의 연마제를 사용하여 최종연마를 행하는 것을 특징으로 하는 합성석영유리기판의 연마방법을 제공한다.Further, the present invention is a method of polishing a synthetic quartz glass substrate having a rough polishing step and a final polishing step after the rough polishing step, wherein in the final polishing step, the synthetic quartz glass substrate of the present invention It provides a method of polishing a synthetic quartz glass substrate, characterized in that the final polishing is performed using an abrasive of.
이러한 본 발명의 합성석영유리기판용의 연마제를 이용한 연마방법이면, 연마속도를 높일 수 있고, 또한, 연마에 의한 결함의 발생을 억제할 수 있다. 이 결과, 대폭 결함이 적은 합성석영유리기판을 효율 좋게 얻을 수 있다.The polishing method using the polishing agent for a synthetic quartz glass substrate according to the present invention can increase the polishing rate and suppress the occurrence of defects due to polishing. As a result, a synthetic quartz glass substrate with significantly fewer defects can be efficiently obtained.
이상과 같이, 본 발명이면, 합성석영유리기판의 최종연마 등에 있어서, 연마속도를 저하시키는 일 없이 합성석영유리기판의 표면의 결함발생을 충분히 억제하는 것이 가능해진다. 그 결과, 합성석영유리기판의 제조에 있어서의, 생산성 및 수율을 향상할 수 있다. 또한, 본 발명의 합성석영유리기판용의 연마제를 사용함으로써, 반도체디바이스의 고정세화(高精細化)로 이어진다.As described above, according to the present invention, it becomes possible to sufficiently suppress the occurrence of defects on the surface of the synthetic quartz glass substrate without reducing the polishing rate in the final polishing of the synthetic quartz glass substrate. As a result, productivity and yield in the production of a synthetic quartz glass substrate can be improved. Further, the use of the polishing agent for the synthetic quartz glass substrate of the present invention leads to high definition of the semiconductor device.
[도 1] 본 발명의 합성석영유리기판의 연마방법에 있어서 사용할 수 있는 연마장치의 일례를 나타내는 개략도이다.Fig. 1 is a schematic diagram showing an example of a polishing apparatus that can be used in the method of polishing a synthetic quartz glass substrate of the present invention.
상술한 바와 같이, 연마속도를 저하시키는 일 없이, 연마에 의한 합성석영유리기판 표면의 결함의 발생을 충분히 저감할 수 있는 합성석영유리기판용의 연마제의 개발이 요구되고 있었다.As described above, there has been a demand for the development of an abrasive for a synthetic quartz glass substrate capable of sufficiently reducing the occurrence of defects on the surface of a synthetic quartz glass substrate due to polishing without lowering the polishing rate.
본 발명자는, 상기 과제에 대하여 예의 검토를 거듭한 결과, 연마입자가 세륨과 이트륨의 복합산화물입자로서, 연마입자 중에 함유되는 세륨의 함유율을 71mol% 이상 79mol% 이하의 범위에서 제조한 입자를 합성석영유리기판용의 연마제에 적용한 결과, 합성석영유리기판을 높은 연마속도로, 또한, 저결함으로 연마할 수 있는 것을 발견하여, 본 발명을 이루었다.The present inventors have repeatedly studied the above problems, and as a result, the abrasive particles are composite oxide particles of cerium and yttrium, and the particles of the cerium contained in the abrasive particles are synthesized in the range of 71 mol% to 79 mol%. As a result of application to an abrasive for a quartz glass substrate, it was found that a synthetic quartz glass substrate can be polished at a high polishing rate and with low defects, and the present invention was achieved.
즉, 본 발명은, 연마입자 및 물을 포함하는, 합성석영유리기판용의 연마제로서, 상기 연마입자가, 세륨과 이트륨의 복합산화물입자로서, 상기 연마입자 중에 함유되는 상기 세륨의 함유율이 71mol% 이상 79mol% 이하인 것을 특징으로 하는 합성석영유리기판용의 연마제이다.That is, the present invention is an abrasive for a synthetic quartz glass substrate containing abrasive particles and water, wherein the abrasive particles are composite oxide particles of cerium and yttrium, and the content of the cerium contained in the abrasive particles is 71 mol%. It is an abrasive for a synthetic quartz glass substrate, characterized in that it is not less than 79 mol%.
이하, 본 발명에 대하여 실시의 형태를 설명하나, 본 발명은 이들로 한정되는 것은 아니다.Hereinafter, embodiments of the present invention will be described, but the present invention is not limited thereto.
상술한 바와 같이, 본 발명의 석영유리기판용의 연마제(이하, 간단히 「연마제」라고도 칭한다.)는, 연마입자 및 물을 포함하고, 연마입자가 세륨과 이트륨의 복합산화물입자로서, 연마입자 중에 함유되는 세륨의 함유량이 71mol% 이상 79mol% 이하이다. 또한, 이 연마입자는, 세륨염을 비롯한 희토류염과 과잉의 알칼리 화합물과의 습식 침전법에 의해 제조된다.As described above, the abrasive for a quartz glass substrate of the present invention (hereinafter, also simply referred to as a "polishing agent") contains abrasive particles and water, and the abrasive particles are composite oxide particles of cerium and yttrium. The content of cerium contained is 71 mol% or more and 79 mol% or less. Further, the abrasive particles are produced by a wet precipitation method of a rare earth salt including a cerium salt and an excess alkali compound.
본 발명의 합성석영유리기판용의 연마제의 연마입자로서, 이러한 연마입자를 사용함으로써, 연마속도를 저하시키는 일 없이 연마에 의한 흠집 등의 결함의 발생을 억제하는 것이 가능해진다.By using such abrasive particles as abrasive particles of the abrasive for a synthetic quartz glass substrate of the present invention, it becomes possible to suppress the occurrence of defects such as scratches due to polishing without lowering the polishing rate.
이하, 각 성분 및 임의로 첨가할 수 있는 성분, 및 본 발명의 연마제에 의한 합성석영유리기판의 연마에 대하여 보다 상세히 설명한다.Hereinafter, each component and components that can be optionally added, and the polishing of the synthetic quartz glass substrate using the abrasive of the present invention will be described in more detail.
일반적으로 합성석영유리기판의 최종연마에 있어서는 실리카입자가 사용되고 있다. 이는 형상이 구형이며 표면이 매끄러운 점에서, 저결함 또한 고평활한 표면이 얻어지기 때문이다. 그러나, 실리카입자는 세리아계 입자와 달리 유리와의 반응성이 낮기 때문에 연마속도는 느려, 연마능력이 있는 연마지립이라고는 하기 어렵다.In general, silica particles are used in the final polishing of synthetic quartz glass substrates. This is because, since the shape is spherical and the surface is smooth, a low defect and high smooth surface is obtained. However, since silica particles have low reactivity with glass, unlike ceria-based particles, the polishing rate is slow, and it is difficult to say that they are abrasive grains having a polishing ability.
유리에 대하여 반응성이 높은 세리아계 입자를 사용함으로써 연마능력을 높이는 것이 가능하나, 실리카입자에 비해 연마에 의한 스크래치 등의 결함이 발생하기 쉽다. 이는 세리아계 입자의 형상이 실리카계 입자에 비해 부정형인 것에 기인함과 함께, 실리카계 입자에 비해 경도가 딱딱한 것이 원인이 된다.Although it is possible to increase the polishing ability by using ceria-based particles having high reactivity with respect to glass, defects such as scratches due to polishing are more likely to occur than silica particles. This is due to the fact that the shape of the ceria-based particles is amorphous compared to the silica-based particles, and is caused by having a harder hardness than the silica-based particles.
이에, 연마입자로서, 세륨염을 비롯한 희토류염과 과잉의 알칼리 화합물과의 습식 침전법에 의해 제조되는 입자를 이용함으로써, 연마속도를 저하시키는 일 없이 연마에 의한 결함의 발생을 저감하는 것이 가능해진다.Accordingly, by using particles produced by wet precipitation of rare earth salts including cerium salts and excess alkali compounds as abrasive particles, it becomes possible to reduce the occurrence of defects due to polishing without lowering the polishing rate. .
본 발명의 연마입자의 평균일차입자경은, 바람직하게는 100nm 내지 500nm, 더욱 바람직하게는 100nm 내지 400nm, 특히 바람직하게는 100nm 내지 300nm이다.The average primary particle diameter of the abrasive particles of the present invention is preferably 100 nm to 500 nm, more preferably 100 nm to 400 nm, and particularly preferably 100 nm to 300 nm.
연마입자의 평균일차입자경이 100nm 이상이면, 석영유리의 연마능력을 충분히 만족시킨다. 또한, 평균일차입자경이 500nm 이하이면, 연마에 의한 스크래치 등의 결함이 발생하는 일도 없다.When the average primary particle diameter of the abrasive particles is 100 nm or more, the polishing ability of the quartz glass is sufficiently satisfied. Further, if the average primary particle diameter is 500 nm or less, defects such as scratches due to polishing do not occur.
본 발명의 연마입자 중의 조성으로는, 세륨의 함유율(함유량)이, 71mol% 이상 79mol% 이하, 더욱 바람직하게는 73mol% 이상 76mol% 이하의 범위로 함으로써, 연마성능이 우수한 연마입자로 할 수 있다.As the composition in the abrasive particles of the present invention, the content (content) of cerium is in the range of 71 mol% or more and 79 mol% or less, more preferably 73 mol% or more and 76 mol% or less, whereby abrasive particles having excellent polishing performance can be obtained. .
연마입자 중에 함유되는 세륨의 함유율이 71mol% 미만이면, 세륨의 함유율이 낮음으로써 연마성능이 저하되는 문제가 발생한다. 또한, 연마입자 중에 함유되는 세륨의 함유율이 79mol%를 초과하면, 제조되는 연마입자의 입경이 커져, 연마에 의한 결함이 발생하기 쉬워지는 문제가 발생한다.If the content of cerium contained in the abrasive particles is less than 71 mol%, the problem of lowering the polishing performance occurs due to the low content of cerium. In addition, when the content of cerium contained in the abrasive particles exceeds 79 mol%, the particle diameter of the produced abrasive particles increases, resulting in a problem that a defect due to polishing is liable to occur.
여기서, 「mol%」란, 세륨과 이트륨의 합계를 100%로 했을 때의 세륨의 값을 말한다.Here, "mol%" refers to the value of cerium when the total of cerium and yttrium is 100%.
입자 중의 희토류원소의 함유량은, 원소분석에 의해 측정이 가능하며, 예를 들어, ICP발광분광플라즈마장치(ICP-AES)에 의해 원소분석이 가능하다.The content of the rare earth element in the particles can be measured by elemental analysis, and elemental analysis can be performed by, for example, an ICP emission spectral plasma apparatus (ICP-AES).
본 발명에서 사용되는 연마입자는, 세륨염을 비롯한 희토류염을 물에 용해한 용액과, 과잉의 알칼리 화합물을 물에 용해한 염기성 용액을 혼합·가열처리하는 습식 침전법에 의해 제조되는 입자인 것이 바람직하다.The abrasive particles used in the present invention are preferably particles produced by a wet precipitation method in which a solution in which rare earth salts including cerium salts are dissolved in water and a basic solution in which an excess alkali compound is dissolved in water is mixed and heated. .
연마입자의 제조방법으로는, 우선, 희토류염으로서 전구체인 질산세륨을 초순수와 혼합하여 세륨용액을 제조한다. 마찬가지로, 희토류염으로서 질산이트륨을 초순수와 혼합하여 이트륨용액을 제조하고, 세륨함유량이 71mol% 이상 79mol% 이하의 범위가 되도록 세륨용액과 혼합하여 세륨이트륨혼합용액을 제조한다.As a method for producing abrasive particles, first, cerium nitrate as a precursor as a rare earth salt is mixed with ultrapure water to prepare a cerium solution. Similarly, yttrium nitrate as a rare earth salt is mixed with ultrapure water to prepare a yttrium solution, and a cerium yttrium mixture solution is prepared by mixing with a cerium solution so that the cerium content is in the range of 71 mol% to 79 mol%.
계속해서, 염기성 용액을 제조한다. 염기성 용액의 알칼리 화합물로는, 요소 또는 요소계의 화합물을 사용할 수 있고, 초순수와 혼합하여 적절한 농도로 조정하여 사용된다. 여기서 요소계 화합물로는, 디메틸아세틸요소, 벤젠설포닐요소, 트리메틸요소, 테트라에틸요소, 테트라메틸요소, 트리페닐요소, 테트라페닐요소 등을 사용할 수도 있다.Subsequently, a basic solution is prepared. As the alkali compound of the basic solution, urea or a urea compound can be used, and it is mixed with ultrapure water and adjusted to an appropriate concentration. Here, as the urea compound, dimethylacetyl urea, benzenesulfonyl urea, trimethyl urea, tetraethyl urea, tetramethyl urea, triphenyl urea, tetraphenyl urea, and the like may be used.
세륨의 함유량을 71mol% 이상 79mol% 이하로 조정한 세륨이트륨혼합용액 중의 이온농도로는, 0.01mol·dm-3 내지 0.1mol·dm-3의 범위로 하는 것이 가능하다. 또한, 세륨이트륨혼합용액에 대하여 과잉의 염기성 용액(알칼리 화합물)을 혼합하나, 염기성 용액 중의 이온농도로는, 세륨이트륨혼합용액의 이온농도의 20~50배의 농도로 하는 것이 바람직하다.The ion concentration in the cerium yttrium mixed solution in which the cerium content is adjusted to 71 mol% or more and 79 mol% or less can be in the range of 0.01 mol·dm -3 to 0.1 mol·dm -3 . In addition, an excess basic solution (alkali compound) is mixed with the cerium yttrium mixed solution, but the ion concentration in the basic solution is preferably 20 to 50 times the ionic concentration of the cerium yttrium mixed solution.
혼합용액의 이온농도 및 염기성 용액의 이온농도를 상기 범위 내로 설정함으로써, 입경이 균일한 입자를 제조할 수 있다.By setting the ionic concentration of the mixed solution and the ionic concentration of the basic solution within the above ranges, particles having a uniform particle diameter can be produced.
다음에, 제조된 세륨용액, 이트륨용액, 염기성 용액을 소정의 혼합비율로 반응용기에 옮긴 후, 교반하고, 소정의 온도로 열처리를 행한다. 이때의 열처리온도는, 100℃ 이하, 예를 들어 80℃ 이상 100℃ 이하의 온도에서 가열처리를 할 수 있고, 열처리시간은, 1시간 이상, 예를 들어 2시간~3시간 행할 수 있다. 또한, 상온에서부터 열처리온도까지의 승온속도는, 매분 3℃~6℃, 바람직하게는 매분 4℃의 속도로 승온할 수 있다.Next, the prepared cerium solution, yttrium solution, and basic solution are transferred to a reaction vessel at a predetermined mixing ratio, stirred, and heat treated at a predetermined temperature. The heat treatment temperature at this time can be performed at a temperature of 100° C. or less, for example 80° C. or more and 100° C. or less, and the heat treatment time may be 1 hour or more, for example, 2 to 3 hours. In addition, the temperature increase rate from room temperature to the heat treatment temperature may be increased at a rate of 3°C to 6°C per minute, preferably 4°C per minute.
열처리를 실시한 혼합용액을, 실온까지 냉각한다. 이러한 과정을 거쳐, 평균일차입자경, 예를 들어 500nm 이하의 세륨과 이트륨의 복합산화물입자가 생성된 혼합액이 제조된다.The heat-treated mixed solution is cooled to room temperature. Through this process, a mixed solution in which composite oxide particles of cerium and yttrium having an average primary particle diameter, for example, 500 nm or less are produced is prepared.
상기와 같이, 본 발명의 연마입자는, 세륨용액과 이트륨용액과 염기성 용액의 혼합액을, 적절한 승온속도로 승온하여, 적절한 범위의 열처리온도로 가열함으로써, 평균일차입자경이 100nm~500nm의 세륨과 이트륨의 복합산화물입자로서 제조된다.As described above, in the abrasive particles of the present invention, a mixture of a cerium solution, a yttrium solution, and a basic solution is heated at an appropriate heating rate and heated to a heat treatment temperature in an appropriate range, so that the average primary particle diameter is 100 nm to 500 nm. It is prepared as a composite oxide particle of.
한편, 본 발명의 연마입자는 소성처리를 행하지 않은 입자인 것이 바람직하다. 이와 같이 소성처리를 행하지 않음으로써, 상술한 건식 세리아입자의 문제를 회피할 수 있다.On the other hand, it is preferable that the abrasive particles of the present invention are particles that have not undergone firing treatment. By not performing the firing treatment in this way, the above-described problem of dry ceria particles can be avoided.
그리고, 본 발명의 합성석영유리기판용의 연마제의 제조방법에서는, 상기와 같이 소정의 희토류염(희토류의 질산염)과 과잉의 알칼리 화합물(요소 또는 요소계의 화합물)과의 습식 침전법에 의해 제조한 연마입자를 물(특히 순수)과 혼합하고, 적당히 하기 첨가제를 첨가하거나, 분산처리 등을 실시하거나 함으로써, 본 발명의 합성석영유리기판용의 연마제를 제조할 수 있다.And, in the manufacturing method of the abrasive for a synthetic quartz glass substrate of the present invention, as described above, it is prepared by a wet precipitation method of a predetermined rare earth salt (rare earth nitrate) and an excess alkali compound (urea or urea compound). By mixing one abrasive particle with water (especially pure water) and appropriately adding the following additives or performing dispersion treatment or the like, the abrasive for a synthetic quartz glass substrate of the present invention can be produced.
본 발명의 연마제에는, 연마특성을 조정하는 목적으로, 첨가제를 함유할 수 있다. 이러한 첨가제로는, 연마입자의 표면전위를 마이너스로 전환할 수 있는 음이온성 계면활성제, 또는 아미노산을 포함할 수 있다. 복합산화물입자의 표면전위를 마이너스로 하면, 연마제 중에서 분산되기 쉬우므로, 입경이 큰 이차입자가 생성되기 어려워, 연마흠집의 발생을 보다 한층 억제할 수 있다.The polishing agent of the present invention may contain an additive for the purpose of adjusting polishing characteristics. As such an additive, an anionic surfactant or an amino acid capable of converting the surface potential of the abrasive particles to negative may be included. When the surface potential of the composite oxide particles is negative, they are easily dispersed in the abrasive, so that secondary particles having a large particle diameter are less likely to be generated, and the occurrence of polishing scratches can be further suppressed.
이러한 첨가제로서의 음이온성 계면활성제에는, 모노알킬황산염, 알킬폴리옥시에틸렌황산염, 알킬벤젠설폰산염, 모노알킬인산염, 라우릴황산염, 폴리카르본산, 폴리아크릴산염, 폴리메타크릴산염 등을 들 수 있다. 아미노산에는, 예를 들어 아르기닌, 라이신, 아스파라긴산, 글루타민산, 아스파라긴, 글루타민, 히스티딘, 프롤린, 티로신, 세린, 트립토판, 트레오닌, 글리신, 알라닌, 메티오닌, 시스테인, 페닐알라닌, 류신, 발린, 이소류신 등을 들 수 있다.Examples of the anionic surfactant as such an additive include monoalkyl sulfate, alkyl polyoxyethylene sulfate, alkylbenzene sulfonate, monoalkyl phosphate, lauryl sulfate, polycarboxylic acid, polyacrylate, and polymethacrylate. Examples of amino acids include arginine, lysine, aspartic acid, glutamic acid, asparagine, glutamine, histidine, proline, tyrosine, serine, tryptophan, threonine, glycine, alanine, methionine, cysteine, phenylalanine, leucine, valine, isoleucine, and the like. .
이들 첨가제를 사용하는 경우의 농도는, 연마입자 1질량부를 기준으로 하여 0.001질량부 내지 0.05질량부의 범위에서 함유하는 것이 바람직하고, 0.005질량부 내지 0.02질량부의 범위에서 함유하는 것이 보다 바람직하다. 함유량이 연마입자 1질량부에 대하여 0.001질량부 이상이면, 연마제 중의 혼합입자가 보다 안정적으로 분산되어, 입경이 큰 응집입자가 형성되기 어려워진다. 또한, 함유량이 연마입자 1질량부에 대하여 0.05질량부 이하이면, 첨가제가 연마를 저해하는 일이 없어, 연마속도의 저하를 방지할 수 있다. 따라서, 상기 범위에서 첨가제를 포함하면, 연마제의 분산안정성을 보다 향상시키는 데다가, 연마속도의 저하를 방지할 수 있다.The concentration in the case of using these additives is preferably contained in a range of 0.001 parts by mass to 0.05 parts by mass, more preferably 0.005 parts by mass to 0.02 parts by mass, based on 1 part by mass of the abrasive particles. When the content is 0.001 parts by mass or more with respect to 1 part by mass of the abrasive particles, the mixed particles in the abrasive are more stably dispersed, and it becomes difficult to form aggregated particles having a large particle diameter. In addition, if the content is 0.05 parts by mass or less based on 1 part by mass of the abrasive particles, the additive does not inhibit polishing, and a decrease in the polishing rate can be prevented. Therefore, when the additive is included in the above range, the dispersion stability of the polishing agent can be further improved, and a decrease in the polishing rate can be prevented.
본 발명의 연마제의 pH는, 연마제의 보존안정성이나, 연마속도가 우수한 점에서, 3.0 이상 8.0 이하의 범위에 있는 것이 바람직하다. pH가 3.0 이상이면 연마제 중의 연마입자가 안정적으로 분산된다. pH가 8.0 이하이면, 연마속도를 보다 향상시키는 것이 가능하다. 또한, pH의 바람직한 범위의 하한은 4.0 이상인 것이 보다 바람직하고, 6.0 이상인 것이 특히 바람직하다. 또한, pH의 바람직한 범위의 상한은, 8.0 이하이며, 7.0 이하인 것이 보다 바람직하다. 또한, 연마제의 pH는, 염산, 질산, 황산, 인산 등의 무기산, 포름산, 아세트산, 구연산, 옥살산 등의 유기산, 암모니아, 수산화나트륨, 수산화칼륨, 테트라메틸암모늄하이드록사이드(TMAH) 등을 첨가함으로써 조정가능하다.The pH of the polishing agent of the present invention is preferably in the range of 3.0 or more and 8.0 or less from the viewpoint of excellent storage stability and polishing rate of the polishing agent. When the pH is 3.0 or higher, the abrasive particles in the abrasive are stably dispersed. If the pH is 8.0 or less, it is possible to further improve the polishing rate. Moreover, it is more preferable that it is 4.0 or more, and, as for the lower limit of a preferable range of pH, it is especially preferable that it is 6.0 or more. Moreover, the upper limit of the preferable range of pH is 8.0 or less, and it is more preferable that it is 7.0 or less. In addition, the pH of the abrasive is by adding inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, organic acids such as formic acid, acetic acid, citric acid, oxalic acid, ammonia, sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide (TMAH), and the like. Is adjustable.
다음에, 본 발명의 연마제를 사용한 합성석영유리기판의 연마방법에 대하여 설명한다. 본 발명의 연마제는 특히 조연마공정 후의 최종연마공정에서 사용하는 것이 바람직하므로, 최종연마공정에 있어서 편면연마를 행하는 경우를 예로 설명한다. 그러나, 물론 이것으로 한정되는 일은 없고, 본 발명의 연마제는 조연마에도 이용할 수 있다. 또한, 본 발명의 연마제는 편면연마뿐만 아니라 양면연마 등에도 이용할 수 있다.Next, a method of polishing a synthetic quartz glass substrate using the polishing agent of the present invention will be described. Since the polishing agent of the present invention is particularly preferably used in the final polishing step after the rough polishing step, a case where single-side polishing is performed in the final polishing step will be described as an example. However, of course, it is not limited to this, and the abrasive of the present invention can also be used for coarse polishing. Further, the abrasive of the present invention can be used not only for single-sided polishing but also for double-sided polishing.
본 발명의 연마방법에 이용할 수 있는 편면연마장치는, 예를 들어, 도 1에 나타낸 바와 같이, 연마패드(4)가 첩부된 정반(3)과, 연마제공급기구(5)와, 연마헤드(2) 등으로 구성된 편면연마장치(10)로 할 수 있다. 또한, 도 1에 나타낸 바와 같이, 연마헤드(2)는, 연마대상인 합성석영유리기판(W)을 유지할 수 있고, 또한, 자전할 수 있다. 또한, 정반(3)도 자전할 수 있다. 연마패드(4)로는, 부직포, 발포폴리우레탄, 다공질 수지 등을 사용할 수 있다. 또한, 연마를 실시하고 있는 동안에는, 항상 연마패드(4)의 표면이 연마제(1)로 덮여 있는 것이 바람직하므로, 연마제공급기구(5)에 펌프 등을 배설함으로써 연속적으로 연마제(1)를 공급하는 것이 바람직하다. 이러한 편면연마장치(10)에서는, 연마헤드(2)로 합성석영유리기판(W)을 유지하고, 연마제공급기구(5)로부터 연마패드(4) 상에 본 발명의 연마제(1)를 공급한다. 그리고, 정반(3)과 연마헤드(2)를 각각 회전시켜 합성석영유리기판(W)의 표면을 연마패드(4)에 슬라이딩접촉시킴으로써 연마를 행한다. 이러한 본 발명의 연마제를 이용한 연마방법이면, 연마속도를 높일 수 있고, 또한, 연마에 의한 결함의 발생을 억제할 수 있다. 그리고, 본 발명의 연마방법은, 대폭 결함이 적은 합성석영유리기판을 얻을 수 있으므로 최종연마에 호적하게 사용할 수 있다.The single-side polishing apparatus that can be used in the polishing method of the present invention is, for example, as shown in Fig. 1, a surface plate 3 to which a
특히 본 발명의 연마방법에 의해 최종연마를 실시한 합성석영유리기판은, 반도체관련의 전자재료(특히 최첨단용도의 반도체관련 전자재료)에 이용할 수 있고, 포토마스크용, 나노임프린트용, 자기디바이스용으로서 호적하게 사용할 수 있다. 한편, 마무리연마 전의 합성석영유리기판은, 예를 들어, 이하와 같은 공정에 의해 준비할 수 있다. 우선, 합성석영유리잉곳을 성형하고, 그 후, 합성석영유리잉곳을 어닐하고, 계속해서, 합성석영유리잉곳을 웨이퍼상으로 슬라이스한다. 계속해서, 슬라이스한 웨이퍼를 면취하고, 그 후, 래핑하고, 계속해서, 웨이퍼의 표면을 경면화하기 위한 연마를 행한다. 그리고 이와 같이 하여 준비한 합성석영유리기판에 대하여, 본 발명의 연마방법에 의해 최종연마를 실시할 수 있다.In particular, the synthetic quartz glass substrate subjected to the final polishing by the polishing method of the present invention can be used for semiconductor-related electronic materials (especially for high-tech semiconductor-related electronic materials), and for photomasks, nanoimprints, and magnetic devices. It can be used suitably. On the other hand, the synthetic quartz glass substrate before finish polishing can be prepared, for example, by the following process. First, a synthetic quartz glass ingot is molded, then, the synthetic quartz glass ingot is annealed, and then the synthetic quartz glass ingot is sliced into a wafer. Subsequently, the sliced wafer is chamfered, followed by wrapping, followed by polishing to mirror the surface of the wafer. Then, the synthetic quartz glass substrate prepared in this way can be subjected to final polishing by the polishing method of the present invention.
실시예Example
이하, 실시예 및 비교예를 이용하여 본 발명을 구체적으로 설명하나, 본 발명은 이것들로 한정되는 것은 아니다.Hereinafter, the present invention will be specifically described using Examples and Comparative Examples, but the present invention is not limited thereto.
[실시예 1][Example 1]
세륨의 이온농도가 71mol%, 이트륨의 이온농도가 29mol%가 되도록, 1mol/l의 질산세륨용액 2.84g과, 1mol/l의 질산이트륨용액 1.16g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 71 mol% and the ion concentration of yttrium is 29 mol%, 2.84 g of 1 mol/l cerium nitrate solution and 1.16 g of 1 mol/l yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixed solution was prepared. Prepared.
계속해서, 5mol/l의 요소용액 48g을 순수 600g으로 희석하여 요소용액을 조제하고, 세륨이트륨혼합용액과 혼합하여 1000g의 반응용액을 조제하였다.Subsequently, 48 g of a 5 mol/l urea solution was diluted with 600 g of pure water to prepare a urea solution, followed by mixing with a cerium yttrium solution to prepare 1000 g of a reaction solution.
조제한 반응용액을 세퍼러블플라스크에 투입하고 반응용액을 90℃에서 2시간 가열교반하여, 반응용액 중에 입자를 석출시켰다.The prepared reaction solution was put into a separable flask, and the reaction solution was heated and stirred at 90° C. for 2 hours to precipitate particles in the reaction solution.
석출된 입자를 원심분리기에 의해 회수하고 건조시킴으로써 연마입자를 얻었다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 71mol%, 이트륨 29mol%였다.The precipitated particles were recovered by a centrifuge and dried to obtain abrasive particles. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 71 mol% of cerium and 29 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 280nm였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 280 nm.
계속해서, 50g의 연마입자를 순수 950g과 혼합하고, 교반하면서 초음파분산처리를 행함으로써 5%의 연마제 1000g을 제조하였다.Subsequently, 50 g of abrasive particles were mixed with 950 g of pure water, and ultrasonic dispersion treatment was performed while stirring to prepare 1000 g of 5% abrasive.
다음에, 이 연마제를 사용하여, 본 발명의 합성석영유리기판의 연마방법에 의해, 도 1에 나타낸 바와 같이 합성석영유리기판(4인치: 100mm)(W)을 연마하였다.Next, using this abrasive, the synthetic quartz glass substrate (4 inches: 100 mm) (W) was polished as shown in Fig. 1 by the method of polishing the synthetic quartz glass substrate of the present invention.
구체적으로는, 연마패드(연질스웨이드제/FILWEL제)(4)를 정반(3)에 첩부하고, 합성석영유리기판(W)의 부착이 가능한 연마헤드(2)에, 조연마를 행한 후의 합성석영유리기판(W)을 세트하고, 연마하중 100gf/cm2, 정반(3) 및 연마헤드(2)의 회전속도를 50rpm, 상기 합성석영유리기판용의 연마제를 매분 100ml로 공급하면서, 조연마공정에서 발생한 결함을 제거하기에 충분한 양으로서 1μm 이상 연마하였다. 연마 후 합성석영유리기판(W)을 연마헤드(2)로부터 분리하고, 순수로 세정 후 다시 초음파세정을 행한 후, 80℃ 건조기로 건조시켰다. 반사분광막두께계(SF-3 오츠카전자(주)제)에 의해, 연마 전후의 합성석영유리기판(W)의 두께 변화를 측정함으로써 연마속도를 산출하였다. 또한, 레이저현미경에 의해, 100nm 이상의 연마 후의 합성석영유리기판(W) 표면에 발생한 결함의 개수를 구하였다. 이 결과, 연마속도는 1.0μm/hr, 결함수는 1개였다.Specifically, a polishing pad (made of soft suede/made of FILWEL) (4) is affixed to the base plate (3), and the synthetic quartz after rough polishing is performed on the polishing head (2) capable of attaching the synthetic quartz glass substrate (W). A glass substrate (W) is set, the polishing load is 100gf/cm 2 , the rotational speed of the platen (3) and the polishing head (2) is 50rpm, and the abrasive for the synthetic quartz glass substrate is supplied at 100ml per minute, while the rough polishing process It was polished by 1 μm or more as an amount sufficient to remove the defects generated in the. After polishing, the synthetic quartz glass substrate (W) was separated from the polishing head (2), washed with pure water, ultrasonically cleaned again, and then dried with a dryer at 80°C. The polishing rate was calculated by measuring the change in the thickness of the synthetic quartz glass substrate W before and after polishing with a reflection spectral film thickness meter (SF-3 manufactured by Otsuka Electronics Co., Ltd.). In addition, the number of defects generated on the surface of the synthetic quartz glass substrate W after polishing of 100 nm or more was determined using a laser microscope. As a result, the polishing rate was 1.0 μm/hr and the number of defects was 1.
[실시예 2][Example 2]
세륨의 이온농도가 78mol%, 이트륨의 이온농도가 22mol%가 되도록, 1mol/l의 질산세륨용액 3.12g과, 1mol/l의 질산이트륨용액 0.88g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 78 mol% and the ion concentration of yttrium is 22 mol%, 3.12 g of 1 mol/l cerium nitrate solution and 0.88 g of 1 mol/l yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 79mol%, 이트륨 21mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 79 mol% cerium and 21 mol% yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 350nm였다. 연마속도는 1.2μm/hr, 결함수는 1개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 350 nm. The polishing rate was 1.2 μm/hr and the number of defects was 1.
[실시예 3][Example 3]
세륨의 이온농도가 73mol%, 이트륨의 이온농도가 27mol%가 되도록, 1mol/l의 질산세륨용액 2.92g과, 1mol/l의 질산이트륨용액 1.08g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 73 mol% and the ion concentration of yttrium is 27 mol%, 2.92 g of 1 mol/l cerium nitrate solution and 1.08 g of 1 mol/l yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 74mol%, 이트륨 26mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 74 mol% of cerium and 26 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 300nm였다. 연마속도는 1.1μm/hr, 결함수는 0개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 300 nm. The polishing rate was 1.1 μm/hr, and the number of defects was 0.
[실시예 4][Example 4]
세륨의 이온농도가 75mol%, 이트륨의 이온농도가 25mol%가 되도록, 1mol/l의 질산세륨용액 3.00g과, 1mol/l의 질산이트륨용액 1.00g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 75 mol% and the ion concentration of yttrium is 25 mol%, 3.00 g of 1 mol/l of cerium nitrate solution and 1.00 g of 1 mol/l of yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 76mol%, 이트륨 24mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 76 mol% of cerium and 24 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 310nm였다. 연마속도는 1.1μm/hr, 결함수는 0개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 310 nm. The polishing rate was 1.1 μm/hr, and the number of defects was 0.
[비교예 1][Comparative Example 1]
세륨의 이온농도가 100mol%가 되도록, 1mol/l의 질산세륨용액 8.00g을 순수로 희석하여 400g의 세륨용액을 조제하였다. 그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다.400 g of a cerium solution was prepared by diluting 8.00 g of 1 mol/l cerium nitrate solution with pure water so that the cerium ion concentration was 100 mol%. Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished.
투과형 전자현미경에 의해 환산한 평균일차입자경은 6500nm였다. 연마속도는 2.5μm/hr, 결함수는 50개였다.The average primary particle diameter converted by a transmission electron microscope was 6500 nm. The polishing rate was 2.5 μm/hr and the number of defects was 50.
[비교예 2][Comparative Example 2]
세륨의 이온농도가 85mol%, 이트륨의 이온농도가 15mol%가 되도록, 1mol/l의 질산세륨용액 3.40g과, 1mol/l의 질산이트륨용액 0.60g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 85 mol% and the ion concentration of yttrium is 15 mol%, 3.40 g of 1 mol/l of cerium nitrate solution and 0.60 g of 1 mol/l of yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 85mol%, 이트륨 15mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 85 mol% of cerium and 15 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 5000nm였다. 연마속도는 2.4μm/hr, 결함수는 48개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 5000 nm. The polishing rate was 2.4 μm/hr and the number of defects was 48.
[비교예 3][Comparative Example 3]
세륨의 이온농도가 80mol%, 이트륨의 이온농도가 20mol%가 되도록, 1mol/l의 질산세륨용액 3.20g과, 1mol/l의 질산이트륨용액 0.80g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 80 mol% and the ion concentration of yttrium is 20 mol%, 3.20 g of 1 mol/l of cerium nitrate solution and 0.80 g of 1 mol/l of yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 80mol%, 이트륨 20mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 80 mol% of cerium and 20 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 4800nm였다. 연마속도는 2.4μm/hr, 결함수는 45개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 4800 nm. The polishing rate was 2.4 μm/hr and the number of defects was 45.
[비교예 4][Comparative Example 4]
이트륨의 이온농도가 100mol%가 되도록, 1mol/l의 질산이트륨용액 8.00g을 순수로 희석하여 400g의 이트륨용액을 조제하였다. 그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다.400 g of yttrium solution was prepared by diluting 8.00 g of 1 mol/l yttrium nitrate solution with pure water so that the yttrium ion concentration was 100 mol%. Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished.
투과형 전자현미경에 의해 환산한 평균일차입자경은 110nm였다. 연마속도는 0.01μm/hr, 결함수는 2개였다.The average primary particle diameter converted by a transmission electron microscope was 110 nm. The polishing rate was 0.01 μm/hr, and the number of defects was two.
[비교예 5][Comparative Example 5]
세륨의 이온농도가 50mol%, 이트륨의 이온농도가 50mol%가 되도록, 1mol/l의 질산세륨용액 2.00g과, 1mol/l의 질산이트륨용액 2.00g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 50 mol% and the ion concentration of yttrium is 50 mol%, 2.00 g of 1 mol/l of cerium nitrate solution and 2.00 g of 1 mol/l of yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 49mol%, 이트륨 51mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 49 mol% cerium and 51 mol% yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 140nm였다. 연마속도는 0.06μm/hr, 결함수는 2개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 140 nm. The polishing rate was 0.06 μm/hr, and the number of defects was two.
[비교예 6][Comparative Example 6]
세륨의 이온농도가 70mol%, 이트륨의 이온농도가 30mol%가 되도록, 1mol/l의 질산세륨용액 2.80g과, 1mol/l의 질산이트륨용액 1.20g을 순수로 희석하여 400g의 세륨이트륨혼합용액을 조제하였다.So that the ion concentration of cerium is 70 mol% and the ion concentration of yttrium is 30 mol%, 2.80 g of 1 mol/l cerium nitrate solution and 1.20 g of 1 mol/l yttrium nitrate solution were diluted with pure water, and 400 g of cerium yttrium mixture was prepared. Prepared.
그리고 실시예 1과 동일한 수순으로 연마제를 제조하여, 합성석영유리기판(W)의 연마를 행하였다. 얻어진 연마입자의 ICP-AES원소분석에 의한 조성비는, 세륨 70mol%, 이트륨 30mol%였다.Then, a polishing agent was prepared in the same procedure as in Example 1, and the synthetic quartz glass substrate W was polished. The composition ratio of the obtained abrasive particles by ICP-AES element analysis was 70 mol% of cerium and 30 mol% of yttrium.
또한, 투과형 전자현미경에 의해 환산한 평균일차입자경은 180nm였다. 연마속도는 0.21μm/hr, 결함수는 2개였다.In addition, the average primary particle diameter converted by the transmission electron microscope was 180 nm. The polishing rate was 0.21 μm/hr, and the number of defects was 2.
상기 실시예 1 내지 4, 비교예 1 내지 6의 결과를 표 1에 나타낸다. 한편, 표 중의 숫자는 각 실시예 및 비교예에서 연마한 합성석영유리기판(W) 5매의 평균값이다.Table 1 shows the results of Examples 1 to 4 and Comparative Examples 1 to 6. On the other hand, the number in the table is the average value of five synthetic quartz glass substrates (W) polished in each Example and Comparative Example.
[표 1][Table 1]
실시예 1 내지 4의 연마제, 즉, 세륨의 비율을 본 발명의 범위 내의 비율로 제조한 연마입자를 사용하여, 합성석영유리기판(W)을 연마한 경우, 연마속도를 저하시키지 않고 연마에 의한 결함의 발생을 적게 억제할 수 있었다.When the synthetic quartz glass substrate (W) was polished using the abrasives of Examples 1 to 4, that is, the abrasive particles in which the ratio of cerium was within the range of the present invention, the polishing was performed without lowering the polishing rate. The occurrence of defects could be suppressed to a small extent.
한편, 세륨의 비율이 소정의 비율보다 높은 비교예 1 내지 3의 연마제에서는, 입경이 커져, 연마 후의 결함수가 증가하였다. 또한, 비교예 4 내지 6의 세륨의 비율이 소정의 비율에 대하여 낮은 연마입자를 사용한 경우는, 입경이 작아 연마속도가 저하되었다.On the other hand, in the abrasives of Comparative Examples 1 to 3 in which the ratio of cerium was higher than the predetermined ratio, the particle diameter increased and the number of defects after polishing increased. In addition, when the abrasive grains in which the ratio of cerium in Comparative Examples 4 to 6 was low relative to a predetermined ratio were used, the grain size was small and the polishing rate was lowered.
이상과 같이, 본 발명의 합성석영유리기판용의 연마제에 의해 합성석영유리기판을 연마함으로써, 합성석영유리기판에 대하여 연마속도를 저하시키지 않고 연마 후의 합성석영유리기판 표면의 결함발생을 충분히 억제시켜 연마할 수 있는 것을 알 수 있었다.As described above, by polishing the synthetic quartz glass substrate with the polishing agent for the synthetic quartz glass substrate of the present invention, the generation of defects on the surface of the synthetic quartz glass substrate after polishing is sufficiently suppressed without lowering the polishing rate for the synthetic quartz glass substrate. I could see what I could polish.
한편, 본 발명은, 상기 실시형태로 한정되는 것은 아니다. 상기 실시형태는 예시이며, 본 발명의 특허청구의 범위에 기재된 기술적 사상과 실질적으로 동일한 구성을 갖고, 동일한 작용효과를 나타내는 것은, 어떠한 것이어도 본 발명의 기술적 범위에 포함된다.In addition, this invention is not limited to the said embodiment. The above-described embodiment is an example, and anything that has substantially the same configuration as the technical idea described in the claims of the present invention and exhibits the same operation and effect is included in the technical scope of the present invention.
Claims (6)
상기 연마입자는 소성처리를 행하지 않은 입자인 것을 특징으로 하는 합성석영유리기판용의 연마제.The method of claim 1,
The abrasive particles for use in synthetic quartz glass substrates, wherein the abrasive particles are particles that have not undergone firing treatment.
상기 연마입자 중에 함유되는 상기 세륨의 함유량이 73mol% 이상 76mol% 이하인 것을 특징으로 하는 합성석영유리기판용의 연마제.The method according to claim 1 or 2,
An abrasive for a synthetic quartz glass substrate, wherein the content of the cerium contained in the abrasive particles is 73 mol% or more and 76 mol% or less.
상기 희토류염을 희토류의 질산염으로 하고, 상기 알칼리 화합물을 요소 또는 요소계의 화합물로 하는 것을 특징으로 하는 합성석영유리기판용의 연마제의 제조방법.The method of claim 4,
A method for producing an abrasive for a synthetic quartz glass substrate, wherein the rare earth salt is used as a rare earth nitrate, and the alkali compound is used as a urea or a urea compound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JPJP-P-2018-083099 | 2018-04-24 | ||
| JP2018083099A JP6936183B2 (en) | 2018-04-24 | 2018-04-24 | Abrasives for synthetic quartz glass substrates and their manufacturing methods, and methods for polishing synthetic quartz glass substrates |
| PCT/JP2019/006198 WO2019207926A1 (en) | 2018-04-24 | 2019-02-20 | Polishing agent for synthetic quartz glass substrates, method for producing same, and method for polishing synthetic quartz glass substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20210003755A true KR20210003755A (en) | 2021-01-12 |
| KR102660018B1 KR102660018B1 (en) | 2024-04-24 |
Family
ID=68293541
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020207030435A KR102660018B1 (en) | 2018-04-24 | 2019-02-20 | Abrasive for synthetic quartz glass substrate, manufacturing method thereof, and polishing method for synthetic quartz glass substrate |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20210162558A1 (en) |
| JP (1) | JP6936183B2 (en) |
| KR (1) | KR102660018B1 (en) |
| CN (1) | CN112004906B (en) |
| TW (1) | TWI785235B (en) |
| WO (1) | WO2019207926A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2021183655A (en) * | 2020-05-21 | 2021-12-02 | 信越化学工業株式会社 | Abrasive agent for polishing synthetic quartz glass substrate and manufacturing method abrasive agent, and polishing method of synthetic quartz glass substrate |
| CN112892809B (en) * | 2021-02-05 | 2023-01-24 | 惠州大唐伟业电子有限公司 | Ultrasonic machining device for optical glass |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004098278A (en) | 2002-08-19 | 2004-04-02 | Hoya Corp | Processes for production of glass substrate for mask blank, mask blank, transfer mask, semiconductor device, glass substrate for mask blank, mask blank and transfer mask |
| JP2007213020A (en) | 2005-12-22 | 2007-08-23 | Asahi Glass Co Ltd | Glass substrate for mask blank and polishing method therefor |
| WO2014208414A1 (en) | 2013-06-27 | 2014-12-31 | コニカミノルタ株式会社 | Cerium oxide abrasive, method for producing cerium oxide abrasive, and polishing method |
| JP5862578B2 (en) | 2011-01-25 | 2016-02-16 | コニカミノルタ株式会社 | Abrasive fine particles and method for producing the same |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3223548B2 (en) * | 1991-11-29 | 2001-10-29 | 日本ビクター株式会社 | Manufacturing method of information glass master |
| WO2009098017A1 (en) * | 2008-02-08 | 2009-08-13 | Umicore | Doped ceria abrasives with controlled morphology and preparation thereof |
| CN101550318B (en) * | 2008-04-03 | 2012-11-14 | 北京有色金属研究总院 | Ce3+ -contained rare-earth polishing powder and preparation method thereof |
| WO2014038536A1 (en) * | 2012-09-05 | 2014-03-13 | コニカミノルタ株式会社 | Production method for polishing-material particles |
| FR2999560B1 (en) * | 2012-12-18 | 2015-01-23 | Saint Gobain Ct Recherches | CRISTALLITE POWDER |
| JP2016092045A (en) * | 2014-10-30 | 2016-05-23 | コニカミノルタ株式会社 | Polishing material, polishing material slurry and polishing treatment method |
| JP2016098351A (en) * | 2014-11-26 | 2016-05-30 | コニカミノルタ株式会社 | Manufacturing method of abrasive agent particle, abrasion agent particle and abrasion agent slurry |
| TWI654288B (en) * | 2015-01-12 | 2019-03-21 | 美商慧盛材料美國責任有限公司 | Composite honing grain for chemical mechanical planarization composition and method of use thereof |
| JP6560155B2 (en) * | 2016-04-20 | 2019-08-14 | 信越化学工業株式会社 | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
| MY190084A (en) * | 2016-08-25 | 2022-03-25 | Shinetsu Chemical Co | Rectangular glass substrate and method for preparing the same |
-
2018
- 2018-04-24 JP JP2018083099A patent/JP6936183B2/en active Active
-
2019
- 2019-02-20 US US17/045,189 patent/US20210162558A1/en active Pending
- 2019-02-20 WO PCT/JP2019/006198 patent/WO2019207926A1/en active Application Filing
- 2019-02-20 KR KR1020207030435A patent/KR102660018B1/en active IP Right Grant
- 2019-02-20 CN CN201980027717.6A patent/CN112004906B/en active Active
- 2019-04-23 TW TW108114065A patent/TWI785235B/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004098278A (en) | 2002-08-19 | 2004-04-02 | Hoya Corp | Processes for production of glass substrate for mask blank, mask blank, transfer mask, semiconductor device, glass substrate for mask blank, mask blank and transfer mask |
| JP2007213020A (en) | 2005-12-22 | 2007-08-23 | Asahi Glass Co Ltd | Glass substrate for mask blank and polishing method therefor |
| JP5862578B2 (en) | 2011-01-25 | 2016-02-16 | コニカミノルタ株式会社 | Abrasive fine particles and method for producing the same |
| WO2014208414A1 (en) | 2013-06-27 | 2014-12-31 | コニカミノルタ株式会社 | Cerium oxide abrasive, method for producing cerium oxide abrasive, and polishing method |
Also Published As
| Publication number | Publication date |
|---|---|
| US20210162558A1 (en) | 2021-06-03 |
| WO2019207926A1 (en) | 2019-10-31 |
| TWI785235B (en) | 2022-12-01 |
| CN112004906B (en) | 2022-03-11 |
| KR102660018B1 (en) | 2024-04-24 |
| JP6936183B2 (en) | 2021-09-15 |
| CN112004906A (en) | 2020-11-27 |
| TW201945509A (en) | 2019-12-01 |
| JP2019189729A (en) | 2019-10-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI712567B (en) | Abrasive for synthetic quartz glass substrate and polishing method for synthetic quartz glass substrate | |
| JP6646062B2 (en) | Polishing agent for synthetic quartz glass substrate, method for producing the same, and method for polishing synthetic quartz glass substrate | |
| CN107532066B (en) | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate | |
| KR102660018B1 (en) | Abrasive for synthetic quartz glass substrate, manufacturing method thereof, and polishing method for synthetic quartz glass substrate | |
| CN110546233B (en) | Polishing agent for synthetic quartz glass substrate, method for producing same, and method for polishing synthetic quartz glass substrate | |
| WO2021235054A1 (en) | Abrasive for synthetic quartz glass substrate, method for producing said abrasive, and method for polishing synthetic quartz glass substrate | |
| TWI779129B (en) | Abrasive for synthetic quartz glass substrate and grinding method for synthetic quartz glass substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E902 | Notification of reason for refusal | ||
| E701 | Decision to grant or registration of patent right |